HRID466220
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
A solution of 4-hydroxy benzonitrile (55 g) in methanol (100 ml) was treated with potassium hydroxide (29 g) in water (30 ml) and evaporated at reduced pressure. The remaining potassium salt was dissolved in dry dimethylformamide (75 ml) and (4R)-2,2-dimethyl-4 - methanesulfonyloxymethyl-1,3-dioxolane, 82.2 g, was add stirring at 110° C. for 20 h, allowed to cool and distributed between ether and water. The aqueous phase was extracted three times with ether, the combined ether phases washed three times with 10% aqueous potassium hydroxide and twice with water, dried over anhydrous sodium sulfate and evaporated. Yield 77 g of the title compound.
WORKUP
后处理
- customevaporated at reduced pressure
- dissolutionThe remaining potassium salt was dissolved in dry dimethylformamide (75 ml)
- addition(4R)-2,2-dimethyl-4 - methanesulfonyloxymethyl-1,3-dioxolane, 82.2 g, was add
- temperatureto cool
- extractionThe aqueous phase was extracted three times with ether
- washthe combined ether phases washed three times with 10% aqueous potassium hydroxide
- dry with materialtwice with water, dried over anhydrous sodium sulfate
- customevaporated